CN104140810A - Manganese-doped barium nitrosilicate luminescence material, and preparation method and application thereof - Google Patents
Manganese-doped barium nitrosilicate luminescence material, and preparation method and application thereof Download PDFInfo
- Publication number
- CN104140810A CN104140810A CN201310168938.XA CN201310168938A CN104140810A CN 104140810 A CN104140810 A CN 104140810A CN 201310168938 A CN201310168938 A CN 201310168938A CN 104140810 A CN104140810 A CN 104140810A
- Authority
- CN
- China
- Prior art keywords
- silicic acid
- basi
- barium salt
- acid barium
- doping nitrogen
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000463 material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 238000004020 luminiscence type Methods 0.000 title abstract description 8
- 229910052788 barium Inorganic materials 0.000 title abstract 4
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 title abstract 4
- 239000000126 substance Substances 0.000 claims abstract description 27
- 239000011159 matrix material Substances 0.000 claims abstract description 13
- 239000011572 manganese Substances 0.000 claims description 69
- -1 nitrogen silicic acid barium salt Chemical compound 0.000 claims description 58
- 229910052748 manganese Inorganic materials 0.000 claims description 57
- 229910016066 BaSi Inorganic materials 0.000 claims description 48
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 46
- 239000000758 substrate Substances 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 25
- 239000012528 membrane Substances 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 16
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 15
- 238000005245 sintering Methods 0.000 claims description 15
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 14
- 238000000137 annealing Methods 0.000 claims description 12
- 150000002696 manganese Chemical class 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000007747 plating Methods 0.000 claims description 6
- 238000004544 sputter deposition Methods 0.000 claims description 6
- 239000010408 film Substances 0.000 abstract description 42
- 239000010409 thin film Substances 0.000 abstract description 6
- 238000001228 spectrum Methods 0.000 abstract description 3
- 230000004913 activation Effects 0.000 abstract 1
- 238000005401 electroluminescence Methods 0.000 abstract 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 15
- 239000001301 oxygen Substances 0.000 description 15
- 229910052760 oxygen Inorganic materials 0.000 description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- 239000011521 glass Substances 0.000 description 11
- 150000002500 ions Chemical class 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 7
- 229960000935 dehydrated alcohol Drugs 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 230000008020 evaporation Effects 0.000 description 7
- 238000001704 evaporation Methods 0.000 description 7
- 238000009832 plasma treatment Methods 0.000 description 7
- 238000004506 ultrasonic cleaning Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000001237 Raman spectrum Methods 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000001194 electroluminescence spectrum Methods 0.000 description 2
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Landscapes
- Luminescent Compositions (AREA)
- Electroluminescent Light Sources (AREA)
Abstract
The chemical formula of a manganese-doped barium nitrosilicate luminescence material is BaSi2O2N2:xMn<4+>, BaSi2O2N2 is a matrix, Mn<4+> is an activation element, and x is 0.01-0.08. In the electroluminescent spectrum (EL) of a luminescence film made by using the manganese-doped barium nitrosilicate luminescence material, a very strong luminescence peak exists in a 520nm wavelength zone, and the luminescence film can be used in thin-film electroluminescence displays. The invention also provides a preparation method and an application of the manganese-doped barium nitrosilicate luminescence material.
Description
[technical field]
The present invention relates to a kind of manganese doping nitrogen silicic acid barium salt luminescent material, its preparation method, manganese doping nitrogen silicic acid barium salt light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof.
[background technology]
Thin-film electroluminescent displays (TFELD), due to its active illuminating, total solids, the advantage such as shock-resistant, reaction is fast, visual angle is large, Applicable temperature is wide, operation is simple, has caused and paid close attention to widely, and development rapidly.At present, research colour and extremely panchromatic TFELD, the luminous material of exploitation multiband, is the developing direction of this problem.But, can be applicable to the manganese doping nitrogen silicic acid barium salt luminescent material of thin-film electroluminescent displays, have not yet to see report.
[summary of the invention]
Based on this, be necessary to provide a kind of manganese doping nitrogen silicic acid barium salt luminescent material, its preparation method, manganese doping nitrogen silicic acid barium salt light-emitting film, its preparation method that can be applicable to membrane electro luminescent device, use membrane electro luminescent device of this manganese doping nitrogen silicic acid barium salt luminescent material and preparation method thereof.
A manganese doping nitrogen silicic acid barium salt luminescent material, its chemical formula is BaSi
2o
2n
2: xMn
4+, BaSi
2o
2n
2matrix, Mn
4+ion is active element, and wherein, x is 0.01～0.08.
Described x is 0.03.
A preparation method for manganese doping nitrogen silicic acid barium salt luminescent material, comprises the following steps:
According to BaSi
2o
2n
2: xMn
4+the stoichiometric ratio of each element takes BaO, SiON and MnO
2powder also mixes, and wherein, x is 0.01～0.08; And
The powder mixing sintering at 900 ℃～1300 ℃ is obtained to chemical formula for 0.5 hour～5 hours is BaSi
2o
2n
2: xMn
4+manganese doping nitrogen silicic acid barium salt luminescent material.
A manganese doping nitrogen silicic acid barium salt light-emitting film, the chemical general formula of the material of this manganese doping nitrogen silicic acid barium salt light-emitting film is BaSi
2o
2n
2: xMn
4+, BaSi
2o
2n
2matrix, Mn
4+ion is active element, and wherein, x is 0.01～0.08.
A preparation method for manganese doping nitrogen silicic acid barium salt light-emitting film, comprises the following steps:
According to BaSi
2o
2n
2: xMn
4+the stoichiometric ratio of each element takes BaO, SiON and MnO
2powder also mixes, and wherein, x is 0.01～0.08;
The vacuum cavity that described target and substrate is packed into magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3pa～1.0 * 10
-5pa; And
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, and underlayer temperature is 250 ℃～750 ℃, is then filmed, and obtaining chemical formula is BaSi
2o
2n
2: xMn
4+manganese doping nitrogen silicic acid barium salt light-emitting film.
Also comprise step: the vacuum annealing at 500 ℃～800 ℃ of described manganese doping nitrogen silicic acid barium salt light-emitting film is processed to 1h～3h.
A kind of membrane electro luminescent device, this membrane electro luminescent device comprises substrate, anode layer, luminescent layer and the cathode layer stacking gradually, the material of described luminescent layer is manganese doping nitrogen silicic acid barium salt luminescent material, and the chemical formula of this manganese doping nitrogen silicic acid barium salt luminescent material is BaSi
2o
2n
2: xMn
4+, BaSi
2o
2n
2matrix, Mn
4+ion is active element, and wherein, x is 0.01～0.08.
A preparation method for membrane electro luminescent device, comprises the following steps:
The substrate with anode is provided;
On described anode, form luminescent layer, the material of described luminescent layer is manganese doping nitrogen silicic acid barium salt luminescent material, and the chemical formula of this manganese doping nitrogen silicic acid barium salt luminescent material is BaSi
2o
2n
2: xMn
4+, BaSi
2o
2n
2matrix, Mn
4+ion is active element, and wherein, x is 0.01～0.08;
On described luminescent layer, form negative electrode.
The preparation of described luminescent layer comprises the following steps:
According to BaSi
2o
2n
2: xMn
4+the stoichiometric ratio of each element takes BaO, SiON and MnO
2powder also mixes sintering at 900 ℃～1300 ℃ and makes target in 0.5 hour～5 hours, and wherein, x is 0.01～0.08;
The vacuum cavity that described target and described substrate is packed into magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3pa～1.0 * 10
-5pa;
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 ℃～750 ℃, then be filmed, on described anode, form luminescent layer.
Also comprise step: the vacuum annealing at 500 ℃～800 ℃ of described manganese doping nitrogen silicic acid barium salt light-emitting film is processed to 1h～3h.
Above-mentioned manganese doping nitrogen silicic acid barium salt luminescent material (BaSi
2o
2n
2: xMn
4+) in the electroluminescent spectrum (EL) of the light-emitting film made, in 520nm wavelength zone, there is very strong glow peak, can be applied in thin-film electroluminescent displays.
[accompanying drawing explanation]
Fig. 1 is the structural representation of the membrane electro luminescent device of an embodiment;
Fig. 2 is the electroluminescent spectrogram of the manganese doping nitrogen silicic acid barium salt light-emitting film of embodiment 1 preparation;
Fig. 3 is the Raman spectrum of the manganese doping nitrogen silicic acid barium salt light-emitting film of embodiment 1 preparation;
Fig. 4 is the voltage of membrane electro luminescent device of embodiment 1 preparation and the graph of relation between current density and voltage and brightness.
[embodiment]
Below in conjunction with the drawings and specific embodiments, manganese doping nitrogen silicic acid barium salt luminescent material, its preparation method, manganese doping nitrogen silicic acid barium salt light-emitting film, its preparation method, membrane electro luminescent device and preparation method thereof are further illustrated.
The manganese doping nitrogen silicic acid barium salt luminescent material of one embodiment, its chemical formula is BaSi
2o
2n
2: xMn
4+, BaSi
2o
2n
2matrix, Mn
4+ion is active element, and wherein, x is 0.01～0.08.
Preferably, x is 0.03.
In the electroluminescent spectrum (EL) of the light-emitting film that this manganese doping nitrogen silicic acid barium salt luminescent material is made, in 520nm wavelength zone, there is very strong glow peak, can be applied in thin-film electroluminescent displays.
The preparation method of above-mentioned manganese doping nitrogen silicic acid barium salt luminescent material, comprises the following steps:
Step S11, according to BaSi
2o
2n
2: xMn
4+the stoichiometric ratio of each element takes BaO, SiON and MnO
2powder also mixes, and wherein, x is 0.01～0.08; And
The powder mixing sintering at 900 ℃～1300 ℃ is obtained to chemical formula for 0.5 hour～5 hours is BaSi
2o
2n
2: xMn
4+manganese doping nitrogen silicic acid barium salt luminescent material.
In this step, preferred, x is 0.03.
Step S12, by mixing equal powder sintering at 900 ℃～1300 ℃, within 0.5 hour～5 hours, can obtain manganese doping nitrogen silicic acid barium salt luminescent material, its chemical formula is BaSi
2o
2n
2: xMn
4+.
In this step, preferred sintering 3 hours at 1250 ℃.
The manganese doping nitrogen silicic acid barium salt light-emitting film of one embodiment, the chemical general formula of the material of this manganese doping nitrogen silicic acid barium salt light-emitting film is BaSi
2o
2n
2: xMn
4+, BaSi
2o
2n
2matrix, Mn
4+ion is active element, and wherein, x is 0.01～0.08.
Preferably, x is 0.03.
The preparation method of above-mentioned manganese doping nitrogen silicic acid barium salt light-emitting film, comprises the following steps:
Step S21, press BaSi
2o
2n
2: xMn
4+the stoichiometric ratio of each element takes BaO, SiON and MnO
2powder also mixes, and wherein, x is 0.01～0.08.
In this step, preferred, x is 0.05, and at 1250 ℃, 3 hours one-tenth diameters of sintering are 50mm, the ceramic target that thickness is 2mm.
Step S22, the target obtaining in step S21 and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3pa～1.0 * 10
-5pa.
In this step, preferred, vacuum tightness is 5 * 10
-4pa.
Step S23, adjustment magnetron sputtering plating processing parameter are: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 ℃～750 ℃; Then be filmed, obtaining chemical formula is BaSi
2o
2n
2: xMn
4+manganese doping nitrogen silicic acid barium salt light-emitting film.
Also comprise step: the vacuum annealing at 500 ℃～800 ℃ of described manganese doping nitrogen silicic acid barium salt light-emitting film is processed to 1h～3h.
In this step, preferred base target spacing is 60mm, magnetron sputtering operating pressure 2Pa, and working gas is oxygen, and the flow of working gas is 25sccm, and underlayer temperature is 500 ℃.
Refer to Fig. 1, the membrane electro luminescent device 100 of an embodiment, this membrane electro luminescent device 100 comprises substrate 1, anode 2, luminescent layer 3 and the negative electrode 4 stacking gradually.
Substrate 1 is glass substrate.Anode 2 is for being formed at the tin indium oxide (ITO) in glass substrate.The material of luminescent layer 3 is manganese doping nitrogen silicic acid barium salt luminescent material, and the chemical formula of this manganese doping nitrogen silicic acid barium salt luminescent material is BaSi
2o
2n
2: xMn
4+, BaSi
2o
2n
2matrix, Mn
4+ion is active element, and wherein, x is 0.01～0.08.The material of negative electrode 4 is silver (Ag).
The preparation method of above-mentioned membrane electro luminescent device, comprises the following steps:
Step S31, provide the substrate 1 with anode 2.
In present embodiment, substrate 1 is glass substrate, and anode 2 is for being formed at the tin indium oxide (ITO) in glass substrate.The substrate 1 with anode 2 is successively with acetone, dehydrated alcohol and deionized water ultrasonic cleaning and use it is carried out to oxygen plasma treatment.
Step S32, on anode 2, form luminescent layer 3, the material of luminescent layer 3 is manganese doping nitrogen silicic acid barium salt luminescent material, and the chemical formula of this manganese doping nitrogen silicic acid barium salt luminescent material is BaSi
2o
2n
2: xMn
4+, BaSi
2o
2n
2matrix, Mn
4+ion is active element, and wherein, x is 0.01～0.08.
In present embodiment, luminescent layer 3 is made by following steps:
First, by BaSi
2o
2n
2: xMn
4+the stoichiometric ratio of each element takes BaO, SiON and MnO
2powder also mixes sintering at 900 ℃～1300 ℃ and makes target in 0.5 hour～5 hours, and wherein, x is 0.01～0.08.
Secondly, target and substrate are packed into the vacuum cavity of magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3pa～1.0 * 10
-5pa.
In this step, preferred, vacuum tightness is 5 * 10
-4pa.
Then, adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 ℃～750 ℃, is then filmed, and forms luminescent layer 3 on anode 2.
In this step, preferred base target spacing is 60mm, magnetron sputtering operating pressure 2Pa, and working gas is oxygen, and the flow of working gas is 25sccm, and underlayer temperature is 500 ℃, and laser energy is 300W.
Also comprise step: the vacuum annealing at 500 ℃～800 ℃ of described manganese doping nitrogen silicic acid barium salt light-emitting film is processed to 1h～3h.
Step S33, on luminescent layer 3, form negative electrode 4.
In present embodiment, the material of negative electrode 4 is silver (Ag), by evaporation, is formed.
Be specific embodiment below.
Embodiment 1
Selecting purity is 99.99% powder, by the BaO of 1mmol, and the SiON of 2mmol and the MnO of 0.03mmol
2powder, after even mixing, at 1250 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 60mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 5.0 * 10
-4pa, the working gas flow of oxygen is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 ℃.The sample chemical formula obtaining is BaSi
2o
2n
2: 0.03Mn
4+light-emitting film, by the light-emitting film obtaining vacuum tightness in vacuum tightness, be then 0.01Pa, annealing temperature is 600 ℃, anneal 2h, evaporation one deck Ag on light-emitting film then, as negative electrode.
The chemical general formula of the manganese doping nitrogen silicic acid barium salt light-emitting film obtaining in the present embodiment is BaSi
2o
2n
2: 0.03Mn
4+.
Refer to Fig. 2, Figure 2 shows that the electroluminescence spectrum (EL) of the manganese doping nitrogen silicic acid barium salt light-emitting film obtaining.As seen from Figure 2, in electroluminescence spectrum, in 520nm wavelength zone, there is very strong glow peak, can be applied in thin-film electroluminescent displays.
Refer to Fig. 3, Fig. 3 is the Raman spectrum of the manganese doping nitrogen silicic acid barium salt light-emitting film of embodiment 1 preparation, Raman peaks is depicted as nitrogen silicic acid barium salt glass characteristic peak as seen from the figure, the peak that does not occur doped element and other impurity, illustrates that doped element and substrate material have formed good bonding.
Refer to Fig. 4, Fig. 4 is the voltage of membrane electro luminescent device of embodiment 1 preparation and the graph of relation between current density and voltage and brightness, curve 1 is voltage and current density relation curve, can find out that this device starts luminous from voltage 5.5V, curve 2 is voltage and brightness relationship curve, and the high-high brightness that can find out this device is 102cd/m
2, show that device has the good characteristics of luminescence.
Embodiment 2
Selecting purity is 99.99% powder, by the BaO of 1mmol, and the SiON of 2mmol and the MnO of 0.08mmol
2powder, after even mixing, at 900 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.5Pa, and underlayer temperature is 250 ℃, and the chemical formula of the sample obtaining is BaSi
2o
2n
2: 0.08Mn
4+light-emitting film, by the light-emitting film obtaining vacuum tightness in vacuum tightness, be then 0.01Pa, annealing temperature is 500 ℃, anneal 1h, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 3
Selecting purity is 99.99% powder, by the BaO of 1mmol, and the SiON of 2mmol and the MnO of 0.01mmol
2powder, after even mixing, at 1300 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 95mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-5pa, the working gas flow of oxygen is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 ℃, and the chemical formula of the sample obtaining is BaSi
2o
2n
2: 0.01Mn
4+light-emitting film, by the light-emitting film obtaining vacuum tightness in vacuum tightness, be then 0.01Pa, annealing temperature is 800 ℃, anneal 3h, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 4
Selecting purity is 99.99% powder, by the BaO of 1mmol, and the SiON of 2mmol and the MnO of 0.06mmol
2powder, after even mixing, at 1250 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 60mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 5.0 * 10
-4pa, the working gas flow of oxygen is 25sccm, and pressure is adjusted to 2.0Pa, and underlayer temperature is 500 ℃, and the chemical formula of the sample obtaining is BaSi
2o
2n
2: 0.06Mn
4+light-emitting film, by the light-emitting film obtaining vacuum tightness in vacuum tightness, be then 0.01Pa, annealing temperature is 600 ℃, anneal 2h, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 5
Selecting purity is 99.99% powder, by the BaO of 1mmol, and the SiON of 2mmol and the MnO of 0.07mmol
2powder, after even mixing, at 900 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 45mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-3pa, the working gas flow of oxygen is 10sccm, and pressure is adjusted to 0.2Pa, and underlayer temperature is 250 ℃, laser energy 500W.The chemical formula of the sample obtaining is BaSi
2o
2n
2: 0.07Mn
4+light-emitting film, by the light-emitting film obtaining vacuum tightness in vacuum tightness, be then 0.01Pa, annealing temperature is 500 ℃, anneal 1h, evaporation one deck Ag on light-emitting film then, as negative electrode.
Embodiment 6
Selecting purity is 99.99% powder, by the BaO of 1mmol, and the SiON of 2mmol and the MnO of 0.04mmol
2powder, after even mixing, at 1300 ℃, sintering diameter into is 50mm, the ceramic target that thickness is 2mm, and target is packed in vacuum cavity.Then, successively use the glass substrate of acetone, dehydrated alcohol and deionized water ultrasonic cleaning band ITO, and use it is carried out to oxygen plasma treatment, put into vacuum cavity.The distance of target and substrate is set as to 95mm.With mechanical pump and molecular pump, the vacuum tightness of cavity is extracted into 1.0 * 10
-5pa, the working gas flow of oxygen is 35sccm, and pressure is adjusted to 4.0Pa, and underlayer temperature is 750 ℃, and the chemical formula of the sample obtaining is BaSi
2o
2n
2: 0.04Mn
4+light-emitting film, by the light-emitting film obtaining vacuum tightness in vacuum tightness, be then 0.01Pa, annealing temperature is 800 ℃, anneal 3h, evaporation one deck Ag on light-emitting film then, as negative electrode.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a manganese doping nitrogen silicic acid barium salt luminescent material, is characterized in that: its chemical formula is BaSi
2o
2n
2: xMn
4+, BaSi
2o
2n
2matrix, Mn
4+ion is active element, and wherein, x is 0.01～0.08.
2. luminescent material according to claim 1, is characterized in that: described x is 0.03.
3. a preparation method for manganese doping nitrogen silicic acid barium salt luminescent material, is characterized in that, comprises the following steps:
According to BaSi
2o
2n
2: xMn
4+the stoichiometric ratio of each element takes BaO, SiON and MnO
2powder also mixes, and wherein, x is 0.01～0.08; And
The powder mixing sintering at 900 ℃～1300 ℃ is obtained to chemical formula for 0.5 hour～5 hours is BaSi
2o
2n
2: xMn
4+manganese doping nitrogen silicic acid barium salt luminescent material.
4. a manganese doping nitrogen silicic acid barium salt light-emitting film, is characterized in that, the chemical general formula of the material of this manganese doping nitrogen silicic acid barium salt light-emitting film is BaSi
2o
2n
2: xMn
4+, BaSi
2o
2n
2matrix, Mn
4+ion is active element, and wherein, x is 0.01～0.08.
5. a preparation method for manganese doping nitrogen silicic acid barium salt light-emitting film, is characterized in that, comprises the following steps:
According to BaSi
2o
2n
2: xMn
4+the stoichiometric ratio of each element takes BaO, SiON and MnO
2powder also mixes, and wherein, x is 0.01～0.08;
The vacuum cavity that described target and substrate is packed into magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3pa～1.0 * 10
-5pa; And
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, and the flow of working gas is 10sccm～35sccm, and underlayer temperature is 250 ℃～750 ℃, is then filmed, and obtaining chemical formula is BaSi
2o
2n
2: xMn
4+manganese doping nitrogen silicic acid barium salt light-emitting film.
6. the preparation method of manganese doping nitrogen silicic acid barium salt light-emitting film according to claim 5, is characterized in that, also comprises step: the vacuum annealing at 500 ℃～800 ℃ of described manganese doping nitrogen silicic acid barium salt light-emitting film is processed to 1h～3h.
7. a membrane electro luminescent device, this membrane electro luminescent device comprises substrate, anode layer, luminescent layer and the cathode layer stacking gradually, it is characterized in that, the material of described luminescent layer is manganese doping nitrogen silicic acid barium salt luminescent material, and the chemical formula of this manganese doping nitrogen silicic acid barium salt luminescent material is BaSi
2o
2n
2: xMn
4+, BaSi
2o
2n
2matrix, Mn
4+ion is active element, and wherein, x is 0.01～0.08.
8. a preparation method for membrane electro luminescent device, is characterized in that, comprises the following steps:
The substrate with anode is provided;
On described anode, form luminescent layer, the material of described luminescent layer is manganese doping nitrogen silicic acid barium salt luminescent material, and the chemical formula of this manganese doping nitrogen silicic acid barium salt luminescent material is BaSi
2o
2n
2: xMn
4+, BaSi
2o
2n
2matrix, Mn
4+ion is active element, and wherein, x is 0.01～0.08;
On described luminescent layer, form negative electrode.
9. the preparation method of membrane electro luminescent device according to claim 8, is characterized in that, the preparation of described luminescent layer comprises the following steps:
According to BaSi
2o
2n
2: xMn
4+the stoichiometric ratio of each element takes BaO, SiON and MnO
2powder also mixes sintering at 900 ℃～1300 ℃ and makes target in 0.5 hour～5 hours, and wherein, x is 0.01～0.08;
The vacuum cavity that described target and described substrate is packed into magnetic-controlled sputtering coating equipment, and the vacuum tightness of vacuum cavity is set to 1.0 * 10
-3pa～1.0 * 10
-5pa;
Adjusting magnetron sputtering plating processing parameter is: base target spacing is 45mm～95mm, magnetron sputtering operating pressure 0.2Pa～4Pa, the flow of working gas is 10sccm～35sccm, underlayer temperature is 250 ℃～750 ℃, then be filmed, on described anode, form luminescent layer.
10. the preparation method of membrane electro luminescent device according to claim 8, is characterized in that, also comprises step: the vacuum annealing at 500 ℃～800 ℃ of described manganese doping nitrogen silicic acid barium salt light-emitting film is processed to 1h～3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310168938.XA CN104140810A (en) | 2013-05-06 | 2013-05-06 | Manganese-doped barium nitrosilicate luminescence material, and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310168938.XA CN104140810A (en) | 2013-05-06 | 2013-05-06 | Manganese-doped barium nitrosilicate luminescence material, and preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104140810A true CN104140810A (en) | 2014-11-12 |
Family
ID=51850153
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310168938.XA Pending CN104140810A (en) | 2013-05-06 | 2013-05-06 | Manganese-doped barium nitrosilicate luminescence material, and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104140810A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020045513A (en) * | 2018-09-18 | 2020-03-26 | 東ソー株式会社 | Barium silicide-based bulk polycrystal and its use |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090050846A1 (en) * | 2006-02-22 | 2009-02-26 | Osram Gesellschaft mit beschränkter Haftung | Illuminant and Light Source Containing the Same, and Method for Producing said Illuminant |
| CN101775292A (en) * | 2010-02-23 | 2010-07-14 | 厦门大学 | Method for preparation of Eu-doped nitrogen oxide phosphor |
| CN102911659A (en) * | 2012-10-15 | 2013-02-06 | 彩虹集团公司 | Nitrogen oxide phosphor powder and synthesis method thereof |
-
2013
- 2013-05-06 CN CN201310168938.XA patent/CN104140810A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090050846A1 (en) * | 2006-02-22 | 2009-02-26 | Osram Gesellschaft mit beschränkter Haftung | Illuminant and Light Source Containing the Same, and Method for Producing said Illuminant |
| CN101775292A (en) * | 2010-02-23 | 2010-07-14 | 厦门大学 | Method for preparation of Eu-doped nitrogen oxide phosphor |
| CN102911659A (en) * | 2012-10-15 | 2013-02-06 | 彩虹集团公司 | Nitrogen oxide phosphor powder and synthesis method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020045513A (en) * | 2018-09-18 | 2020-03-26 | 東ソー株式会社 | Barium silicide-based bulk polycrystal and its use |
| JP7167578B2 (en) | 2018-09-18 | 2022-11-09 | 東ソー株式会社 | Barium silicide-based bulk polycrystal and its use |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102863957B (en) | Manganese-chromium-doped zinc tungstate luminescent material and preparation method and application thereof | |
| CN102863959B (en) | Europium-doped gadolinium molybdate luminescent material, preparation method and application thereof | |
| CN104673298A (en) | Samarium-doped alkaline-earth niobium zincate luminescent material, and preparation method and application thereof | |
| CN104140810A (en) | Manganese-doped barium nitrosilicate luminescence material, and preparation method and application thereof | |
| CN104140813A (en) | Manganese-chromium-codoped silicon-aluminium oxynitride alkaline-earth salt luminescent material, preparation method and application thereof | |
| CN104178148A (en) | Antimony and terbium co-doped alkali niobate luminescent material, and preparation method and application thereof | |
| CN103421496B (en) | Manganese Ti doped fluorine magnesium germanate luminescence material, preparation method and applications | |
| CN104178160A (en) | Cerium terbium double-doped nitrogen silicon lanthanum luminescent material and preparation method and application thereof | |
| CN103788948A (en) | Europium-terbium-codoped rare earth silicate luminescent material, and preparation method and application thereof | |
| CN102863956B (en) | Praseodymium-doped barium titanate luminescent material and preparation method and application thereof | |
| CN104342158A (en) | Europium-erbium double-doped zinc selenide luminescent material, and preparation method and application thereof | |
| CN103571475A (en) | Titanium manganese-codoped group-III molybdate luminescent material, preparation method and application thereof | |
| CN103571477A (en) | Europium bismuth co-doped Group-III molybdate light-emitting material, preparation method and application thereof | |
| CN104140812A (en) | III-group scandium silicate luminescent material co-doped with titanium and manganese, preparing method thereof and applications of the material | |
| CN103571468A (en) | Antimony terbium co-doped silicon aluminum nitrogen oxide light-emitting material and preparation method and application thereof | |
| CN104140815A (en) | Samarium-doped rare earth gallate luminescent material, preparing method thereof and applications of the material | |
| CN103421509B (en) | Cerium dopping vanadium yttrium phosphate salt luminescent material, preparation method and application thereof | |
| CN104140817A (en) | Europium-terbium-codoped rare-earth aluminate luminescent material, preparation method and application thereof | |
| CN104119896A (en) | Manganese and titanium co-doped arsenate luminescent material and preparation method and application thereof | |
| CN104650918A (en) | Europium- bismuth- co-doped IIIA-group yttrium fluoride luminescent materials, and preparing method and applications thereof | |
| CN104119906A (en) | Antimony terbium co-doped silicon nitride luminescent material and preparation method and application thereof | |
| CN104650909A (en) | Manganese-doped cerium pentaphosphate luminescent material, and preparation method and application thereof | |
| CN104673282A (en) | Manganese-chromium/codoped alkaline-earth zincate luminescent material, and preparation method and application thereof | |
| CN104650902A (en) | Manganese-doped arsenic acid cerium luminescent material, preparation method and application thereof | |
| CN104650869A (en) | Europium- terbium- co-doped aluminium niobate luminescent materials, and preparing method and applications thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141112 |